CN112724459B - Preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agent - Google Patents

Preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agent Download PDF

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CN112724459B
CN112724459B CN202011589791.8A CN202011589791A CN112724459B CN 112724459 B CN112724459 B CN 112724459B CN 202011589791 A CN202011589791 A CN 202011589791A CN 112724459 B CN112724459 B CN 112724459B
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CN112724459A (en
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王铁刚
左桂福
王丹丹
刘文财
王红霞
李�浩
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Tangshan Boshide Medical Devices Co ltd
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    • C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/048—Elimination of a frozen liquid phase
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    • C08J2205/00—Foams characterised by their properties
    • C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/022—Hydrogel, i.e. a gel containing an aqueous composition
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    • C08J2207/00—Foams characterised by their intended use
    • C08J2207/12—Sanitary use, e.g. diapers, napkins or bandages
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    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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    • C08J2301/28—Alkyl ethers
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    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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    • C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
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    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
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    • C08K3/16—Halogen-containing compounds

Abstract

The invention provides a preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agent, which comprises the following steps: (1) preparing a high-molecular aqueous solution; (2) preparing an antibacterial liquid; (3) preparing an antibacterial sponge; (4) preparing a hydrogel solution; (5) and (3) preparation of the antibacterial hydrogel. The method can realize the uniform dispersion of the antibacterial agent, and can realize the controllable release of the antibacterial component through the regulation and control of the components and the proportion of the water-soluble high polymer material. The composite hydrogel prepared by the invention has better antibacterial stability and antibacterial durability, and the porous sponge can realize higher water locking and mechanical enhancement effects.

Description

Preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agent
Technical Field
The invention relates to the field of biomedical materials, in particular to a preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agents.
Background
The medical hydrogel has semi-permeability, and has the effects of blocking bacteria, preventing wound infection, allowing oxygen and water to pass through, and the like.
Practice proves that the hydrogel has a better promoting effect on the recovery of the wound than the conventional dressing, but the water in the hydrogel is easy to breed bacteria, and blood and tissue fluid at the wound are also easy to breed bacteria to cause infection. Therefore, in order to inhibit bacterial growth and reduce the probability of wound infection, it is important to develop hydrogel with antibacterial function.
At present, the conventional antibacterial hydrogel technology is mainly divided into intrinsic antibacterial hydrogel and additive antibacterial hydrogel. Most of the intrinsic antibacterial hydrogel is a high molecular material with antibacterial property such as chitosan, and the antibacterial efficiency of the technology is limited. The addition type antibacterial hydrogel is prepared by adding an antibacterial agent into a hydrogel matrix by a blending method, and the technology easily causes the dispersion and the release of the antibacterial agent to be nonuniform and uncontrollable, so that the antibacterial efficiency and the service cycle of the antibacterial hydrogel are influenced.
The invention adopts a two-step method to prepare the antibacterial hydrogel with uniformly dispersed and controllable release of the antibacterial agent.
Disclosure of Invention
In view of this, the invention provides a preparation method of an antibacterial hydrogel with uniformly dispersed and controllable release of an antibacterial agent. The method can realize the uniform dispersion of the antibacterial agent, and can realize the controllable release of the antibacterial component through the regulation and control of the components and the proportion of the water-soluble high polymer material.
The preparation method of the antibacterial hydrogel with the uniformly dispersed and controllable release antibacterial agent, provided by the invention, comprises the following steps:
(1) preparing a high-molecular water solution: dissolving water-soluble polymer in deionized water to prepare polymer aqueous solution with mass concentration of 0.5-5 wt%;
(2) preparation of antibacterial liquid: weighing the polymer aqueous solution obtained in the step (1), adding an antibacterial agent, and stirring at normal temperature for 0.5-2h and at the stirring speed of 100-;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 0.5-5h, and freezing the antibacterial liquid into a state of ice-water mixture; then freeze-drying for 30-40h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the water-soluble polymer solution in the step (1), and adding 0.1-1 wt% of cross-linking agent to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: and (3) soaking the antibacterial sponge in the hydrogel solution in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature at room temperature for 0.5-3h, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel.
Preferably, the water-soluble polymer material in step (1) is one or more of sodium carboxymethyl cellulose, polyvinyl alcohol, carboxymethyl chitosan, sodium alginate and gelatin.
Preferably, the antibacterial agent in step (2) is any one of nano zinc oxide, nano titanium oxide, nano silver and chlorine dioxide precursor.
Preferably, the mass ratio of the antibacterial agent to the high polymer material in the step (2) is 0.1: 10-3: 10.
Preferably, the freezing condition in the freeze dryer in the step (3) is-50 ℃ and the vacuum degree is 20 Pa.
Preferably, in the step (4), the cross-linking agent is any one of calcium chloride, glutaraldehyde, genipin and borax.
The preparation method of the antibacterial hydrogel with the uniformly dispersed and controllable release antibacterial agent, provided by the invention, adopts a two-step method to prepare the antibacterial hydrogel with the uniformly dispersed and controllable release antibacterial agent. Firstly, adding an antibacterial agent into a water-soluble polymer solution, and preparing the polymer antibacterial porous sponge by freeze drying or other pore-forming technologies. And secondly, impregnating the antibacterial sponge with the prepared hydrogel liquid to form the antibacterial hydrogel.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the antibacterial hydrogel with the uniformly dispersed and controllable release antibacterial agent can realize the uniform dispersion of the antibacterial agent and simultaneously realize the controllable release of the antibacterial component through the regulation and control of the components and the proportion of the water-soluble high polymer material. The prepared composite hydrogel has good antibacterial stability and antibacterial durability, and the porous sponge can realize higher water locking and mechanical enhancement effects.
Drawings
FIG. 1 is a schematic view showing a method for preparing an antibacterial hydrogel in which an antibacterial agent is uniformly dispersed and controllably released.
Detailed Description
The following examples are provided to further illustrate the preparation method of the antibacterial hydrogel with the uniformly dispersed and controlled release antibacterial agent.
Example 1
A preparation method of antibacterial hydrogel with uniformly dispersed and controllable release antibacterial agent comprises the following steps:
(1) preparing a high-molecular water solution: dissolving water-soluble high-molecular sodium carboxymethylcellulose in deionized water to prepare a high-molecular aqueous solution with the mass concentration of 2 wt%;
(2) preparation of antibacterial liquid: weighing 100mL of the polymer aqueous solution obtained in the step (1), adding 10g of antibacterial agent nano zinc oxide, and stirring at normal temperature for 1h at the stirring speed of 500r/min to obtain an antibacterial liquid;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 3 hours to be frozen into a state of ice-water mixture; then, under the conditions of-50 ℃ and 20Pa of vacuum degree, carrying out freeze drying for 30h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the water-soluble polymer solution prepared in the step (1), and adding 0.5wt% of cross-linking agent glutaraldehyde to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: and (3) soaking the antibacterial sponge prepared in the step (3) in the hydrogel solution prepared in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature for 2 hours at room temperature, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel.
Example 2
(1) Preparing a high-molecular water solution: dissolving sodium alginate in deionized water to prepare a macromolecular aqueous solution with the mass concentration of 1 wt%;
(2) preparation of antibacterial liquid: weighing 100mL of the high polymer aqueous solution obtained in the step (1), adding 5g of chlorine dioxide precursor sodium chlorite of an antibacterial agent, and stirring at normal temperature for 1h at the stirring speed of 800r/min to obtain antibacterial liquid;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 3 hours to be frozen into a state of ice-water mixture; then, under the conditions of-50 ℃ and 20Pa of vacuum degree, carrying out freeze drying for 30h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the water-soluble polymer solution prepared in the step (1), and adding 1wt% of cross-linking agent calcium chloride to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: and (3) soaking the antibacterial sponge prepared in the step (3) in the hydrogel solution prepared in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature for 2 hours at room temperature, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel.
Example 3
(1) Preparing a high-molecular water solution: dissolving chitosan in deionized water to prepare a high-molecular water solution with the mass concentration of 5 wt%;
(2) preparation of antibacterial liquid: weighing 100mL of the polymer aqueous solution obtained in the step (1), adding 0.1g of antibacterial agent nano silver, and stirring at normal temperature for 1h at the stirring speed of 500r/min to obtain antibacterial liquid;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 3 hours to be frozen into a state of ice-water mixture; then, under the conditions of-50 ℃ and 20Pa of vacuum degree, carrying out freeze drying for 30h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the water-soluble polymer solution prepared in the step (1), and adding 0.5wt% of cross-linking agent glutaraldehyde to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: and (3) soaking the antibacterial sponge prepared in the step (3) in the hydrogel solution prepared in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature for 2 hours at room temperature, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel.
Example 4
(1) Preparing a high-molecular water solution: dissolving polyvinyl alcohol in deionized water to prepare a high-molecular water solution with the mass concentration of 2 wt%;
(2) preparation of antibacterial liquid: weighing 100mL of the polymer aqueous solution obtained in the step (1), adding 30g of antibacterial agent nano titanium oxide, and stirring at normal temperature for 1h at the stirring speed of 500r/min to obtain antibacterial liquid;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 3 hours to be frozen into a state of ice-water mixture; then, under the conditions of-50 ℃ and 20Pa of vacuum degree, carrying out freeze drying for 30h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the water-soluble polymer solution prepared in the step (1), and adding 0.5wt% of cross-linking agent glutaraldehyde to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: and (3) soaking the antibacterial sponge prepared in the step (3) in the hydrogel solution prepared in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature for 2 hours at room temperature, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (4)

1. A preparation method of antibacterial hydrogel with uniformly dispersed and controllable release of antibacterial agent is characterized by comprising the following steps:
(1) preparing a high-molecular water solution: dissolving a water-soluble polymer material in deionized water to prepare a polymer aqueous solution with the mass concentration of 0.5-5 wt%;
(2) preparation of antibacterial liquid: weighing the polymer aqueous solution obtained in the step (1), adding an antibacterial agent, and stirring at normal temperature for 0.5-2h and at the stirring speed of 100-;
(3) preparing an antibacterial sponge: freezing the antibacterial liquid prepared in the step (2) at the temperature of below 0 ℃ for 0.5-5h, and freezing the antibacterial liquid into a state of ice-water mixture; then freeze-drying for 30-40h in a freeze dryer to prepare the antibacterial sponge;
(4) preparing a hydrogel solution: weighing the polymer aqueous solution in the step (1), and adding 0.1-1 wt% of cross-linking agent to obtain a hydrogel solution;
(5) preparing the antibacterial hydrogel: soaking the antibacterial sponge in the step (3) in the hydrogel solution in the step (4), removing bubbles by adopting a vacuum bubble removal mode, keeping the temperature at room temperature for 0.5-3h, and completing hydrogel crosslinking and curing to obtain the antibacterial hydrogel;
the mass ratio of the antibacterial agent to the water-soluble polymer material in the step (2) is 0.1: 10-3: 10;
the freezing condition in the freeze dryer in the step (3) is that the temperature is minus 50 ℃ and the vacuum degree is 20 Pa.
2. The method for preparing the antibacterial hydrogel with the uniformly dispersed and controlled release antibacterial agent according to claim 1, wherein the water-soluble polymer material in the step (1) is one or more of sodium carboxymethylcellulose, polyvinyl alcohol, carboxymethyl chitosan, sodium alginate and gelatin.
3. The method for preparing the antibacterial hydrogel with the uniformly dispersed and controlled release antibacterial agent according to claim 1, wherein the antibacterial agent in the step (2) is any one of nano zinc oxide, nano titanium oxide, nano silver and chlorine dioxide precursor.
4. The method for preparing the antibacterial hydrogel with the uniformly dispersed and controlled release antibacterial agent according to claim 1, wherein the cross-linking agent in the step (4) is any one of calcium chloride, glutaraldehyde, genipin and borax.
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